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111.
Blagg RJ López-Gómez MJ Charmant JP Connelly NG Cowell JJ Haddow MF Hamilton A Orpen AG Riis-Johannessen T Saithong S 《Dalton transactions (Cambridge, England : 2003)》2011,40(43):11497-11510
The structures of [{RhLL'(μ-X)}(2)] [LL' = cod, (CO)(2), (CO)(PPh(3)) or {P(OPh)(3)}(2); X = mt or taz], prepared from [{RhLL'(μ-Cl)}(2)] and HX in the presence of NEt(3), depend on the auxiliary ligands LL'. The head-to-tail arrangement of the two N,S-bridges is accompanied by a rhodium-eclipsed conformation for the majority but the most hindered complex, [{Rh[P(OPh)(3)](2)(μ-taz)}(2)], uniquely adopts a sulfur-eclipsed structure. The least hindered complex, [{Rh(CO)(2)(μ-mt)}(2)], shows intermolecular stacking of mt rings in the solid state. The complexes [{RhLL'(μ-X)}(2)] are chemically oxidised to trinuclear cations, [(RhLL')(3)(μ-X)(2)](+), most probably via reaction of one molecule of the dimer, in the sulfur-eclipsed form, with the fragment [RhLL'](+) formed by oxidative cleavage of a second. 相似文献
112.
Baber RA Orpen AG Pringle PG Wilkinson MJ Wingad RL 《Dalton transactions (Cambridge, England : 2003)》2005,(4):659-667
The coordination chemistry of the four phosphines, P{C6H3(o-CH3)(p-Z)}3 where Z = H (1a) or OMe (1b) and P{C6H3(o-CHMe2)(p-Z)}3 Z = H (1c) or OMe (1d) with platinum(II) and palladium(II) is reported. Mononuclear complexes trans-[PdCl2L2](L = 1a,b) and trans-[PtCl2L2](L = 1a-c) have been prepared and the crystal structures of trans-[PdCl2(1b)2] and trans-[PtCl2(1c)2] as their dichloromethane solvates have been determined. The structures show that in these complexes, the ligands adopt g+ g+ a conformations. Examination of the Cambridge Structural Database confirms this to be one of only two conformer types that tri-o-tolylphosphines adopt and the only viable conformer in 4 and 6 coordinate complexes. The binuclear complexes trans-[Pd2Cl4L2](L = 1c,d) are formed even when an excess of the bulky 1c,d is used in the synthesis and the crystal structure of trans-[Pd2Cl4(1c)2] as its chloroform solvate is reported. Reaction of [PtCl2(NCBu(t))2] with 1b-d in refluxing toluene gave the cycloplatinated species [Pt2Cl2(L - H)2] where L - H is phosphine 1b-d deprotonated at one of the ortho-methyl carbon atoms. Variable temperature 31P and 1H NMR spectroscopy reveals that all the complexes reported are fluxional. The processes are analysed in terms of restricted P-C and P-M rotations that give rise to diastereoisomeric rotamers because of the helically chiral orientations of the aryl substituents. For the complexes of the bulky ligands 1c,d, rotation about the P-C bond is slow on the NMR timescale even up to 75 degrees C. The crystal structure of the cyclometallated complex [Pt2Cl2(1d - H)2] has been determined. 相似文献
113.
Neil G. Connelly Thomas Escher Antonio J. Martin Bernhard Metz A. Guy Orpen 《Journal of Cluster Science》1995,6(1):125-134
Treatment of [W(CO)(MeC2Me)2(-C5H5)][PF6] with ONMe3 in acetonitrile yields [W(NCMe)(MeC2Me)2(-C5H5)][PF6] which undergoes irreversible reduction at a Pt electrode in THF. Sodium amalgam reduction of [W(NCMe) (MeC2Me)2(-C5H5)][PF6] gives orange crystals of [W2(µ-,,
2,
2-C4Me4)2 (-C5H5)2] X-ray studies on which reveal pairwise alkyne coupling and a novel bis(metallacyclopentadiene) structure.Dedicated to Professor L. F. Dahl on the occasion of his 65th birthday. 相似文献
114.
Baya M Houghton J Konya D Champouret Y Daran JC Almeida Leñero KQ Schoon L Mul WP van Oort AB Meijboom N Drent E Orpen AG Poli R 《Journal of the American Chemical Society》2008,130(32):10612-10624
Reduction of compound "Pd(bcope)(OTf)2" [bcope = (c-C8H14-1,5)PCH2CH2P(c-C8H14-1,5); OTf = O3SCF3] with H2/CO yields a mixture of Pd(I) compounds [Pd2(bcope)2(CO)2](OTf)2 (1) and [Pd2(bcope)2(mu-CO)(mu-H)](OTf) (2), whereas reduction with H2 or Ph3SiH in the absence of CO leads to [Pd3(bcope)3(mu3-H)2](OTf)2 (3). Exposure of 3 to CO leads to 1 and 2. The structures of 1 and 3 have been determined by X-ray diffraction. Complex [Pd2(bcope)2(CO)2](2+) displays a metal-metal bonded structure with a square planar environment for the Pd atoms and terminally bonded CO ligands and is fluxional in solution. DFT calculations aid the interpretation of this fluxional behavior as resulting from an intramolecular exchange of the two inequivalent P atom positions via a symmetric bis-CO-bridged intermediate. A cyclic voltammetric investigation reveals a very complex redox behavior for the "Pd(bcope)(OTf)2"/CO system and suggests possible pathways leading to the formation of the various observed products, as well as their relationship with the active species of the PdL2(2+)/CO/H2-catalyzed oxo processes (L2 = diphosphine ligands). 相似文献
115.
Sin C. James Yvonne G. Lawson Nicholas C. Norman A. Guy Orpen Michael J. Quayle 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(4):427-429
Two pentahalo(N‐donor)bismuthate(III) salts, bis[hydrogen bis(4‐picoline)(1+)] pentabromo(4‐picoline‐N)bismuthate(III), (C12H15N2)2[BiBr5(C6H7N)], (I), and bis(pyridinium) pentachloro(pyridine‐N)bismuthate(III), (C5H6N)2[BiCl5(C5H5N)], (II), are described which show modest deviations from octahedral geometry at bismuth. In (I), the cations comprise two 4‐picoline molecules sharing a proton and in (II), pyridinium cations are present. The anion in (I) has twofold and that in (II) has mirror crystallographic symmetry. Both structures show a layered packing formed by the anions with the cations between the layers. Ring–ring interactions seem important in (I), whilst in (II), N/C—H?Cl—Bi hydrogen bonding is abundant. 相似文献